Chapter 4 - Liquid - Liquid Extraction PDF
Chapter 4 - Liquid - Liquid Extraction PDF
PART 4.1
Explain the basic concepts of single and multistage of
liquid-liquid extraction.
Able to draw ternary phase diagram, locate and read
the composition of mixture on the diagram.
Use ternary phase diagram and equation for calculate
the composition of the product from liquid-liquid
extraction for single and multistage liquid-liquid
extraction.
For example : Mixture of water & vinegar will produced
homogenous mixture
Mixture of water & oil will produced heterogeneous mixture
When C
Component mixed with
A will A & B, C
separate will pull
form B away A
from B
Miscible
solvent C
or
immiscible
or partially
miscible
Extraction
Washing acid & in Purification of
base industry uranium
If the constituents of a liquid solution have close
boiling points or close vapor pressures.
If the constituents of a liquid solution have relative
volatility near unity (1).
If the distillation utilizes an excessive amount of
steam.
If the constituents of a liquid solution form an
azeotropic mixture or non-ideal mixture
If one or more of the components involved is sensitive
to heat.
Main disadvantages is that the extract phase has to be
treated further (usually by distillation) in order to
separate A from the solvent.
OCT 2012
State the guidelines when separation using
liquid-liquid extraction method is preferred
over the distillation method.
(5 marks)
C
Solvent
A and C
Extract layer
A and B
solution
A and B
Raffinate layer
A and C Extract layer
Extract layer • Mainly C, extracted A and dissolved B
Raffinate layer
A and B • Mainly B, leftover A and dissolved C
Raffinate layer
Raffinate layer
A and B • Mainly B and leftover A
Raffinate layer
APEX
100 % A
TIE LINE
RAFFINATE P
EXTRACT
HALF-DOME W HALF-DOME
Q
Z
R RIGHT
LEFT CORNER
CORNER 100 % C
100 % B B C
A,B & C = Solute A, solution B & solvent C
TIE LINE WZ = Connect the left dome & the right dome & connect
the equilibrium compositions of the raffinate & extract phases
i. 100 % EG
ii. 100 % furfural
iii. 100 % water
iv. Tie line
v. F
vi. S
vii. Solvent-free raffinate
viii. Mass fraction of EG
ix. Mass fraction furfural
x. R
20,000 kg/h feed solution, F containing 42 wt% EG, 50 wt% water
& 8 wt% Furfural. Locate this mixture on triangular diagram
F
SOLUTION
Horizontal axis = Mass fraction of Furfural (draw vertical
line through 0.08)
Vertical axis = Mass fraction of EG (draw horizontal line
through 0.42)
SOLUTION
Furfural act as solvent, basis = 100g extract
Solvent-free weight fraction of EG = 32/(32+8)
= 0.8
Solvent-free weight fraction of water = 8/(32+8)
= 0.2
Thus, solvent-free composition of the extract, ESF = 80% EG,
20%
water
2. Draw a straight line from
3.The intersection of this blue
100% furfural through point E
line with EG-water line gives the
to the EG-water line
solvent free composition , ESF
ESF
1. Locate point E on
triangular diagram.
E Point E is a intersection
between horizontal &
RSF vertical axis
1. Identify which component are the solute A,
diluent B, & the solvent C
2. If want to position C on the right corner,
must locate points for the ternary phase
diagram using weight fractions of C on
horizontal axis & weight fractions of A on
vertical axis
3. Normally, ternary equilibrium data are given
on raffinate-extract pair
4. Once draw these points pair-wise, need to
draw tie-lines connecting raffinate & extract
6500 kg/h of an acetone-MIBK solution containing 25 wt%
acetone is counter-currently extracted with water to reduce
acetone concentration to 5% (solvent-free). Draw a right-angle
triangular ternary phase diagram for an MIBK-acetone-water
given the following equilibrium data
SOLUTION
1. Acetone = solute A, water as solvent C, MIBK as diluent B
2. Acetone must be on apex vertical axis, water can be horizontal
axis
3. Locate points on diagram using weight fractions of water &
acetone only, draw them pair by pair to obtain the correct tie
lines
MIBK-acetone-water system
0.900
0.800
0.700
0.600
Data from MIBK rich
layer (raffinate phase) Data from water rich
0.500 layer (extract phase)
0.400
0.300
0.200
0.100
0.000
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800 0.900 1.000
MIBK water
PART 2.2
Solvent & solution Raffinate & extract
are in contact each are in equilibrium
other only once only once
At equilibrium, rate
of A from B to C
=from C to B
E, Extract phase
F, feed y* A
solution
xF A
Single-stage M, intermediate
S, extracting liquid-liquid
extraction xM A
solvent
yS A
R, Raffinate phase
x* A
Where,
F is mass of feed solution in kg, or Ibm
S is mass of extracting solvent in kg or Ibm
E is mass of an extract phase in kg or Ibm
R is mass of a raffinate phase in kg or Ibm
M is mass of a raffinate phase in kg or Ibm
x is mass fraction of solute A in solution with B
y is mass fraction of solute A in solution with extracting
solvent C
xM is mass fraction of solute A in intermediate phase.
x* is equilibrium mass fraction of solute A raffinate phase
y* is equilibrium mass fraction of solute A in extract phase.
Using material balance,
Calculate the mass of intermediate M using total material
balance:
F + S = M
Determine mass fraction of solute A in intermediate M using
material balance for solute A:
xF.F + yS.S = M.xM
xM = (xF.F + yS.S) / M
Using the value of
xM, locate point M on
Draw a straight
Locate points F the FS line. Note
line from F to
and S. that that point M
S.
MUST be on the FS
line.
From the new tie line,
Draw a line that pass locate point E and
through point M. This point R and hence
new tie line must determine the
take shape of the composition of
nearest given tie raffinate, R, and
lines. extract, E that are in
equilibrium.
SOLUTION
Use the following equilibrium tie-line data 250C & 101 kPa 9in
weight %) to construct the ternary phase diagram
Flow diagram for the process :
xM = 40/200 = 0.2
1
0.9
0.8
0.7
0.6
0.5
F
0.4
0.3 E
M
0.2
0.1
R
S
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Locate points F & S
Using calculated value xM = 0.2, locate point M on the FS line. Point M MUST
be on the FS line
Draw a new tie line that pass through point M. This new tie line must take
shape of the nearest tie lines
From new tie line, can locate point E & R, determine the composition of
raffinate, R & extract E
a) From point E, extract phase contains 0.26 mass fraction of EG
From point R, raffinate phase contains 0.075 mass fraction of EG
b) Using material balance :
Total mass balance : F + S = R + E = 200…………………….(1)
EG mass balance : xF.F + xS.S = x*R + y*E
0.4(100) + 0 = 0.075R + 0.26E
40 = 0.075R + 0.26E………….(2)
E = 135.3 kg, R = 64.9 kg
If we use lever rule :
Length of RM = 4.8 cm
Length of ER = 7.0 cm
Mass of extract E = Length of RM/Length of ER x mass of
intermediate M
= (4.8/7.0) x 200
= 137.1 kg
Mass of raffinate R = Mass of intermediate M – Mass of extract E
= 200 – 137.1
= 67.9 kg
c) % EG extracted = mass of EG in extract/mass of EG in feed x 100 %
a) A mixture containing 33 wt% acetic acid, 2 wt%
isopropyl ether & 65 wt% water is treated with equal
weight of recycled solvent which contains 3 wt%
acetic acid in a simple one stage batch extraction
i. What are the solvent-free compositions & weights of
the raffinate & extract layers
ii. Calculate the percent extraction of acetic acid by
isopropyl ether
b. If the raffinate layer from the above treatment is
extracted again with half its weight of solvent, what
will be the solvent-free compositions of new layers?
1.00
Acetic acid
0.90
0.80 E1SF
0.70
0.60
0.50
0.40
F
0.30 R1SF
R1 M
0.20
E1
0.10
S
Isopropylether
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
0.80
0.70
0.60
0.50
0.40
0.30
0.20
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
0.80
0.70
0.60 Point F
0.50
0.40
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
0.80
0.70
0.60 Point F
0.50
Point M
0.40
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
0.80
0.70
0.60 Point F
0.50
Point M
0.40
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
0.80
0.70
0.60 Point F
0.50
Point R1
Point M
0.40
Point E1
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
1.00
Acetic acid
0.90
E1sf
0.80
0.70
0.60 Point F
0.50
Point R1
Point M
0.40
Point E1
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
E11.00
sf
Acetic acid
0.90
E1sf
0.80
0.70
R1sf
0.60 Point F
0.50
Point R1
Point M
0.40
Point E1
0.30
0.20
Point S
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
SOLUTION
Calculate the mass of intermediate M using total material
balance : F + S = M, 100 + 100 = M
Determine mass fraction of solute in intermediate M using
material balance for solute (acetic acid) :
0.33(100) + 0.03(100) = M.xM
xM = 36/200 = 0.18
To determine solvent-free composition of extract E1, construct a
straight line from 100 % solvent (ether) through point E1 to the
acetic acid-water binary side. Thus the solvent-free composition
of extract as given by point E1SF is 76 % acetic acid. The solvent-
free composition of raffinate is given by point R1SF = 0.27
Total mass balance :
F + S = R + E = 200………..(1)
Total mass balance EG :
xF.F + xS.S = x*R + y*E
0.33(100) + 0 = 0.26R + 0.13E
33 = 0.26R + 0.13E…………….(2)
Substitute E = 200 – R into (2)
33 = 0.26R + 0.13(200 – R)
33 = 0.26R + 26 – 0.13R
0.26R – 0.13R = 33 – 26
0.13R = 7
R = 53.85 kJ/kg, E = 146.15 kJ/kg
(ii) % of extraction acid = y*.E/xF.F x 100 %
= 0.13 x 146.15/0.33 x 100 x 100 %
= 18.9995/33 x 100 % = 57.57 %
OCT 2012
A mixture containing 30 wt% acetic acid and 70 wt % water is
treated
with equal weight of recycled solvent which contains 4 wt %
acetic acid in
a simple one stage batch extraction. Using acetic acid-water-
isopropyl
ether phase diagram in Appendix 2,
i. Calculate M and xM
ii. Determine the solvent-free compositions of the extract
phase and raffinate phase
iii. Determine the composition of raffinate and extract phase
iv. Calculate the weight of the raffinate and extract phase
1.00
Acetic acid
0.90
0.80
0.70
0.60
0.50
0.40
0.30
0.20
0.10
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
PART 2.3
Solvent and solution come into contact more than
once. The solvent and the solution, which flow
opposite (countercurrent) to each other, mix on
stages inside an extractor.
Resulting extracts and raffinates are in equilibrium.
Sincethey are many stages inside an extractors, the
extracts and the raffinates will reach equilibrium
more than once.
F kg/h feed solution E kg/h final extract
xF A yE A
Stage 1
Stage 2
Stage 3
Stage 4
Stage n-2
Stage n -1
Stage n
Stage n+1
Rn-1 kg/h diluent-rich phase from stage n-1 En kg/h solvent-rich phase from stage n
yn* A
xn-1 A
Stage n
En+1 kg/h solvent-rich phase from stage n+1 Rn kg/h diluent-rich phase from stage n
yn+1 A xn* A
When
accumulated A in
Solvent rich- Mass transfer
solvent-rich
phase (En+1) from occur (A More A
reaches a certain
stage n+1 and molecules from molecules are
limit,
diluent-rich phase the diluent-rich accumulating in
accumulated A in
(Rn-1) from stage phase migrate to the solvent-rich-
solvent-rich
n-1 mix on stage the solvent-rich phase
phase starts
n phase)
returning back to
diluent-rich phase
Rate of A
Mass fraction of transferring from
A in equilibrium diluent-rich phase
Out-flowing new New diluent-rich
diluent-rich = xn* to solvent-rich
diluent-rich (Rn) & phase and
& mass fraction phase = rate of A
solvent-rich (En) solvent-rich
of A in transferring from
phases are in phase emerge
equilibrium solvent-rich
equilibrium from the stage n.
solvent-rich = phase back to
yn*. diluent-rich
phase.
R2 kg/h diluent-rich phase from stage n-1 E3 kg/h solvent-rich phase from stage n
y3* A
x2 A
Stage 3
S4 kg/h solvent-rich phase from stage n+1 R3 kg/h diluent-rich phase from stage n
y4 A x3* A
Stage n-2
Stage n -1
Stage n
Stage n+1
S = 1500 kg/h extracting solvent R kg/h raffinate
yS = 0 xR = 0.02 (solvent free)
21. Now have 2 data set to draw Mac-Cabe diagram, firstly draw equilibrium
curve, follow by operating line & finally step up from bottom to
determine the number of ideal stages. Each step represents an ideal
stages
1
0.9
0.8
0.7
0.6
E
0.5
0.4
F
0.3 M
0.2
0.1
Rsf R S
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
0.6
Equilibrium curve
0.5
1
0.4
2
0.3
y
Operating Line
0.2 3
0.1
Draw best tie lines originate from F. Intersection of this line with extract half-
dome is point Emin
Intersection of this line with FS gives point Mmin. From point Mmin can read value
of xMmin
Stage 1
Stage 2
Stage 3
Stage 4
Stage n-2
Stage n -1
Stage n
Stage n+1
0.8
0.7
0.6
Emin
0.5
0.4
0.3
F
Mmin
0.2 x
min
0.1Rsf
R
S
0
0 water 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 Furfural 1
0.600
Equilibrium curved
0.500
0.400
Number of ideal stages = 2
0.300
y
1
0.200
Operating line
0.100
2
0.000
0.000 0.100 0.200 0.300 0.400 0.500 0.600
x